CN102021653B - Method for growing silicon carbide single crystal by using high-density material block - Google Patents
Method for growing silicon carbide single crystal by using high-density material block Download PDFInfo
- Publication number
- CN102021653B CN102021653B CN 201010615255 CN201010615255A CN102021653B CN 102021653 B CN102021653 B CN 102021653B CN 201010615255 CN201010615255 CN 201010615255 CN 201010615255 A CN201010615255 A CN 201010615255A CN 102021653 B CN102021653 B CN 102021653B
- Authority
- CN
- China
- Prior art keywords
- silicon carbide
- crucible
- single crystal
- density
- material block
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000000463 material Substances 0.000 title claims abstract description 46
- 239000013078 crystal Substances 0.000 title claims abstract description 32
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 16
- 229910052799 carbon Inorganic materials 0.000 claims description 11
- 229910003978 SiClx Inorganic materials 0.000 claims description 10
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000007770 graphite material Substances 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- 239000011863 silicon-based powder Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 abstract description 12
- 239000012535 impurity Substances 0.000 abstract description 4
- 239000004065 semiconductor Substances 0.000 abstract description 3
- 238000012546 transfer Methods 0.000 abstract description 2
- 230000005540 biological transmission Effects 0.000 abstract 1
- 239000007792 gaseous phase Substances 0.000 abstract 1
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004891 communication Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a method for growing a silicon carbide single crystal by using a high-density material block, belonging to the technical field of the preparation of semiconductor materials. The method comprises the steps of: (1) preparing a high-density silicon carbide material block, (2) underlaying the high-density silicon carbide material block in the step (1) with a cushion block to ensure that the material block is not in contact with a crucible, and placing the material block at the bottom of the crucible to be used as a raw material, and (3) placing a seed crystal at the top of the crucible, and growing the silicon carbide single crystal with a physical gaseous phase transmission method. The method solves the problem that powder is in direct contact with the crucible and realizes radiative heat transfer between the inner wall of the crucible and the aerial material block, the grown single crystal is uniform and symmetrical, and the content of impurities in the single crystal is greatly reduced.
Description
Technical field
The present invention relates to a kind of method of growing silicon carbide single crystal, belong to the semiconductor material preparing technical field.
Background technology
Single-crystal silicon carbide is as semiconductor material with wide forbidden band, have excellent physical properties and the electrical properties such as high heat conductance, high breaking down field strength, high saturated electrons drift speed, have huge application prospect in fields such as aerospace, seafari, radar communication, automotive electronics.
Growing silicon carbide single crystal generally adopts the physical vapor transport method at present, be that raw material is sublimed into gaseous substance in the high-temperature zone, gaseous substance is transferred under the effect of thermograde with the raw material surface seed crystal face certain distance, that temperature is lower, and crystallizes into bulk crystals on seed crystal.
The general raw material that adopts of this kind method is sic powder, or carbon dust, silica flour etc., all belongs to powder, therefore directly contacts with the crucible inwall, belongs to the direct heat conduction.Affected by the relative position of crucible in ruhmkorff coil larger, and between powder, thermal conductivity is relatively poor, eel-like figure shape or taper in the middle of clout is generally, and outside greying is serious.And using the powder growth easily to introduce impurity, impurity is evaporated to seed crystal face in the high growth temperature process, cause various lattice defects.
Summary of the invention
The technical problem to be solved in the present invention is the defective that overcomes existing growing silicon carbide single crystal method, provides a kind of monocrystalline of growth even, symmetrical, the growing silicon carbide single crystal method that purity is high.
In order to solve the problems of the technologies described above, the invention provides following technical scheme:
A kind of method with the high-density material block growing silicon carbide single crystal, step be,
(1) preparation high density carbon SiClx material piece,
(2) the high density carbon SiClx material piece with step (1) paves with cushion block, and the material piece is not contacted with crucible, and be placed in crucible bottom as raw material,
(3) seed crystal is placed at the crucible top, uses the physical vapor transport growing silicon carbide single crystal.
Further, the raw material of described preparation high density carbon SiClx material piece can be but be not limited to be silicon carbide abrasive, high-pure SiC power, high pure carbon powder, high-purity silicon powder.
Or/and cylindrical grinder is processed, its upper and lower surface is parallel, and diameter is slightly less than the crucible internal diameter through surface grinding machine for described high density carbon SiClx material piece.
Described high density carbon SiClx material piece is single-crystal silicon carbide piece, polycrystalline agglomerate or pressure caking, and its volume density is not less than 1.5g/cm
3Single-crystal silicon carbide density is 3.2g/cm
3, namely required material piece density is approximately greater than half of monocrystalline density, and material piece density is got over the people, and its heat conductivility is better, and internal temperature is more even.
The height of described cushion block is adjusted according to the crucible degree of depth, material tile height, charge level and seed crystal spacing, and scope is between 5mm-60mm, in order to keep required charge level and seed crystal to ask apart from (generally remaining between 10-50mm).
Described cushion block can be but be not limited to be graphite material.
In the inventive method, the material piece paves with materials such as graphite blocks in the bottom, and leave certain interval between the crucible inwall, make it directly not contact with crucible, just the conduction of the direct heat between powder in original crucible inwall and crucible is become the radiative transfer of asking of crucible inwall and " making somebody a mere figurehead " material piece, the material piece is subjected to a temperature inhomogeneous impact less in crucible, and because the material piece is finer and close than powder, thermal conductivity increases greatly, therefore in the piece material, temperature is even, symmetry is very good, and the monocrystalline that is conducive to grow is even, symmetrical.And because the growth of each crystal or high temperature sintering have impurities removal, purification effect, so grow in advance or the material piece of sintering is equivalent to through primary purification with powder, foreign matter content wherein reduces greatly, is conducive to reduce the defective in monocrystalline.
Embodiment
Below the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein only is used for description and interpretation the present invention, is not intended to limit the present invention.
Embodiment 1:
As raw material, expect high 100mm with the sic powder of particle diameter 0.6mm, crucible is placed in suitable position, growth temperature is controlled at 2000-2300 ℃, is filled with Ar gas to 200Pa, grows to get monocrystalline material piece (being designated as material piece 1) after 24 hours, high 35mm, diameter 72mm; Grow in the same way again and to get polycrystal piece (be designated as and expect piece 2), high 30mm, diameter 72mm.The long-pending density of two material blocks is 3.2 g/cm
3, but aufwuchsplate is uneven, after surface grinding machine and cylindrical grinder processing, and the high 33mm of material piece 1, the high 26mm of material piece 2.Two material pieces are placed on the graphite cushion block (diameter 20mm, height 60mm) of crucible bottom and make raw material, use the physical vapor transport growing silicon carbide single crystal.The high 26mm of gained crystal, diameter 78mm, symmetry is good, single product foreign matter content low (than better with single product transparency of growing under the powder similarity condition).
Embodiment 2:
As raw material, press that to form volume density be 1.5 g/cm with the sic powder of particle diameter 0.05mm by the method that waits static pressure
3The material piece.Three these kinds material pieces are placed on the graphite cushion block (diameter 30mm, highly be 5mm) of crucible bottom, use the physical vapor transport growing silicon carbide single crystal.The high 20mm of gained crystal, diameter 78mm, symmetry is good, monocrystalline foreign matter content low (than better with the single crystal transparent degree of growing under the powder similarity condition).
It should be noted that at last: the above only is the preferred embodiments of the present invention, be not limited to the present invention, although with reference to previous embodiment, the present invention is had been described in detail, for a person skilled in the art, it still can be modified to the technical scheme that aforementioned each embodiment puts down in writing, and perhaps part technical characterictic wherein is equal to replacement.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., within all should being included in the protection domain of wood invention.
Claims (3)
1. method with the high-density material block growing silicon carbide single crystal is characterized in that: step is,
(1) preparation high density carbon SiClx material piece,
(2) the high density carbon SiClx material piece with step (1) paves with cushion block, and the material piece is not contacted with crucible, and be placed in crucible bottom as raw material,
(3) seed crystal is placed at the crucible top, uses the physical vapor transport growing silicon carbide single crystal;
Wherein, described high density carbon SiClx material piece is single-crystal silicon carbide piece, polycrystalline agglomerate or pressure caking, and its volume density is 1.5-3.2g/cm
3Described cushion block is graphite material, and the height of described cushion block is adjusted according to the crucible degree of depth, material tile height, charge level and seed crystal spacing, and scope is between 5mm-60mm.
2. the method with the high-density material block growing silicon carbide single crystal according to claim 1, it is characterized in that: the raw material of described preparation high density carbon SiClx material piece is silicon carbide abrasive, high-pure SiC power, high pure carbon powder, high-purity silicon powder.
3. the method with the high-density material block growing silicon carbide single crystal according to claim 1 is characterized in that: or/and cylindrical grinder processing, its upper and lower surface is parallel, and diameter is slightly less than the crucible internal diameter through surface grinding machine for described high density carbon SiClx material piece.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010615255 CN102021653B (en) | 2010-12-30 | 2010-12-30 | Method for growing silicon carbide single crystal by using high-density material block |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010615255 CN102021653B (en) | 2010-12-30 | 2010-12-30 | Method for growing silicon carbide single crystal by using high-density material block |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102021653A CN102021653A (en) | 2011-04-20 |
| CN102021653B true CN102021653B (en) | 2013-06-12 |
Family
ID=43863417
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010615255 Active CN102021653B (en) | 2010-12-30 | 2010-12-30 | Method for growing silicon carbide single crystal by using high-density material block |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102021653B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3922762A4 (en) * | 2020-04-14 | 2022-01-05 | Meishan Boya Advanced Materials Co., Ltd. | Crystal growth method and device |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105543965A (en) * | 2016-02-02 | 2016-05-04 | 北京华进创威电子有限公司 | Crucible structure used for silicon carbide single crystal growth |
| CN106480503B (en) * | 2016-12-09 | 2018-11-20 | 河北同光晶体有限公司 | A kind of growing method of granular carbonization silicon single crystal |
| CN108624963A (en) * | 2018-05-16 | 2018-10-09 | 福建北电新材料科技有限公司 | A kind of raw material sintering process of carborundum crystals for the growth of PVT methods |
| JP7242978B2 (en) | 2018-11-26 | 2023-03-22 | 株式会社レゾナック | Manufacturing method of SiC single crystal ingot |
| CN111962152A (en) * | 2020-09-14 | 2020-11-20 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Preparation method of silicon carbide single crystal for reducing crystal defects |
| CN113622029B (en) * | 2021-08-12 | 2022-11-29 | 山东天岳先进科技股份有限公司 | Crucible assembly having polycrystalline block, method of manufacturing the same, and silicon carbide single crystal manufactured therefrom |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1367275A (en) * | 2001-01-20 | 2002-09-04 | 上海德波赛康科研有限公司 | Preparation method of block silicone carbide monocrystal growth |
| CN1544715A (en) * | 2003-11-14 | 2004-11-10 | 中国科学院物理研究所 | Method and apparatus for growing silicon carbide single crystal by physical vapor transportation |
| CN101701358A (en) * | 2009-11-25 | 2010-05-05 | 中国科学院上海硅酸盐研究所 | Method for preparing high-quality large silicon carbide single crystal and silicon carbide single crystal prepared by same |
| CN101812723A (en) * | 2010-04-20 | 2010-08-25 | 中国科学院上海硅酸盐研究所 | Method and device for growing silicon carbide signal crystals based on physical vapor transport technology |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4225296B2 (en) * | 2005-06-20 | 2009-02-18 | トヨタ自動車株式会社 | Method for producing silicon carbide single crystal |
| JP5250321B2 (en) * | 2008-07-04 | 2013-07-31 | 昭和電工株式会社 | Method for producing seed crystal for silicon carbide single crystal growth and method for producing silicon carbide single crystal |
-
2010
- 2010-12-30 CN CN 201010615255 patent/CN102021653B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1367275A (en) * | 2001-01-20 | 2002-09-04 | 上海德波赛康科研有限公司 | Preparation method of block silicone carbide monocrystal growth |
| CN1544715A (en) * | 2003-11-14 | 2004-11-10 | 中国科学院物理研究所 | Method and apparatus for growing silicon carbide single crystal by physical vapor transportation |
| CN101701358A (en) * | 2009-11-25 | 2010-05-05 | 中国科学院上海硅酸盐研究所 | Method for preparing high-quality large silicon carbide single crystal and silicon carbide single crystal prepared by same |
| CN101812723A (en) * | 2010-04-20 | 2010-08-25 | 中国科学院上海硅酸盐研究所 | Method and device for growing silicon carbide signal crystals based on physical vapor transport technology |
Non-Patent Citations (2)
| Title |
|---|
| 姜守振等.沿[1100]方向升华法生长6H－SiC单晶.《人工晶体学报》.2007,第36卷(第1期),14-17. * |
| 陈之战等.原料对碳化硅单晶生长的影响.《无机材料学报》.2003,第18卷(第4期),737-743. * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3922762A4 (en) * | 2020-04-14 | 2022-01-05 | Meishan Boya Advanced Materials Co., Ltd. | Crystal growth method and device |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102021653A (en) | 2011-04-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102021653B (en) | Method for growing silicon carbide single crystal by using high-density material block | |
| CN104805504B (en) | A kind of method of fast-growth large size silicon-carbide monocrystalline | |
| TWI613335B (en) | Method for producing tantalum carbide powder and tantalum carbide single crystal | |
| CN105463580A (en) | Preparation method of cadmium selenide or cadmium sulfide two-dimensional monocrystal nanosheet | |
| CN103708463B (en) | The preparation method of feather weight high-pure SiC power | |
| CN1282770C (en) | Device and method for growng large diameter 6H-SiC monocrystal with semiconductor property | |
| CN106968018A (en) | A kind of growing method for the single-crystal silicon carbide material that germanium nitrogen is co-doped with | |
| CN102732953A (en) | Technology and apparatus for growing single silicon carbide crystals through double seed crystal-assisted vapor transport method | |
| CN108624963A (en) | A kind of raw material sintering process of carborundum crystals for the growth of PVT methods | |
| CN110016718A (en) | A kind of processing method for growing silicon carbide crystal with high quality feedstock purification | |
| CN104828825A (en) | Low-cost method for synthesizing silicon carbide powder at low temperature | |
| CN102425008A (en) | Method for preparing large-grain ingot polycrystal silicon | |
| CN102978694A (en) | Improved kyropoulos method for sapphire crystal growth | |
| CN103184512A (en) | Silicon carbide single crystal growing apparatus with regulatable axial-temperature gradient | |
| CN108946735B (en) | Synthesis method of large-particle-size silicon carbide powder for silicon carbide crystal growth | |
| CN114182357A (en) | Method for regrowing silicon carbide single crystal by using broken crystal grains of silicon carbide crystal | |
| CN109576783A (en) | A kind of preprocessing method of raw materials for high quality aluminum nitride crystal growth | |
| CN107522489B (en) | Preparation method of polycrystalline SnSe thermoelectric material | |
| CN111962152A (en) | Preparation method of silicon carbide single crystal for reducing crystal defects | |
| TWI675946B (en) | Device for growing carbides of a specific shape | |
| Tao | Bulk gallium oxide single crystal growth | |
| CN204325549U (en) | A kind of silicon carbide crystal growing device | |
| CN106591952A (en) | Preparation method of SiC wafer | |
| CN116119670A (en) | Preparation method of ultralow N, B content silicon carbide raw material | |
| JP6829767B2 (en) | Manufacturing method and manufacturing equipment for SiC raw materials for SiC crystal growth |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Application publication date: 20110420 Assignee: CENTURY GOLDRAY SEMICONDUCTOR CO., LTD. Assignor: Beijing Huajin Chuangwei Electronics Co., Ltd. Contract record no.: 2015110000045 Denomination of invention: Method for growing silicon carbide single crystal by using high-density material block Granted publication date: 20130612 License type: Exclusive License Record date: 20151103 |
|
| LICC | Enforcement, change and cancellation of record of contracts on the licence for exploitation of a patent or utility model | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Method for growing silicon carbide single crystal by using high-density material block Effective date of registration: 20151117 Granted publication date: 20130612 Pledgee: Medium range Leasing Co. Ltd. Pledgor: Beijing Huajin Chuangwei Electronics Co., Ltd. Registration number: 2015990001011 |
|
| PLDC | Enforcement, change and cancellation of contracts on pledge of patent right or utility model | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20161201 Granted publication date: 20130612 Pledgee: Medium range Leasing Co. Ltd. Pledgor: Beijing Huajin Chuangwei Electronics Co., Ltd. Registration number: 2015990001011 |
|
| PLDC | Enforcement, change and cancellation of contracts on pledge of patent right or utility model | ||
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20170109 Address after: Tonghui trunk road 100176 Beijing city Daxing District economic and Technological Development Zone No. 17 hospital Patentee after: CENTURY GOLDRAY SEMICONDUCTOR CO., LTD. Address before: 100176 Beijing economic and Technological Development Zone, Beijing, sea road, No. 17, No. three, No. Patentee before: Beijing Huajin Chuangwei Electronics Co., Ltd. |
|
| PP01 | Preservation of patent right |
Effective date of registration: 20180814 Granted publication date: 20130612 |
|
| PP01 | Preservation of patent right | ||
| PD01 | Discharge of preservation of patent |
Date of cancellation: 20200810 Granted publication date: 20130612 |
|
| PD01 | Discharge of preservation of patent |